JPS62230636A - Production of porous glass article - Google Patents
Production of porous glass articleInfo
- Publication number
- JPS62230636A JPS62230636A JP7326186A JP7326186A JPS62230636A JP S62230636 A JPS62230636 A JP S62230636A JP 7326186 A JP7326186 A JP 7326186A JP 7326186 A JP7326186 A JP 7326186A JP S62230636 A JPS62230636 A JP S62230636A
- Authority
- JP
- Japan
- Prior art keywords
- porous glass
- particles
- glass article
- synthesized
- sol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000005373 porous glass Substances 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000003980 solgel method Methods 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims abstract description 3
- 150000004703 alkoxides Chemical class 0.000 claims abstract 3
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 17
- 239000011521 glass Substances 0.000 abstract description 9
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 4
- 239000004327 boric acid Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/108—Forming porous, sintered or foamed beads
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は多孔質ガラス体の製造方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for manufacturing a porous glass body.
従来の多孔質ガラスの製造方法はコーニングク。 The conventional manufacturing method for porous glass is Koninguk.
ラスワークス社の特許（Ｕ 、Ｓ 、Ｐａｔ ２２１５
０５９．２２２１７０９）に示されるように、硼酸・ア
ルカリ金属酸化物、珪砂等を主原料として溶融した硼珪
酸ガラスを、数百度の温度で熱処理して珪砂質のガラス
相と、硼酸とアルカリ金属酸化物に富んだガラス相とに
分相させる。次にこのガラスを酸溶液、又は熱水で処理
することにより、硼酸とアルカリ金ｍＫ富んだガラス相
を溶出させ、珪酸成分に富んだ元の形状を保持したガラ
スを得るという方法であった〇
〔発明が解決しようとする問題点〕
しかし前述の従来技術では、硼酸とアルカリ金ｊｉｌｌ
Ｋ富んだガラス相を溶出させることにより細孔を形成す
るため、数センチメートルに及ぶ厚さのガラスについて
゛は均一な細孔を形成することが不可能であり・又・バ
ルク状のものは得ることが困難であるという問題点を有
する。そこで本発明はこのような問題点を解決するもの
で、その目的とするところは数センチメートルの厚さの
バルク状であり均一な細孔を有し、しかも分布が非常に
シャープである多孔質ガラスの製造方法を提供するとこ
ろｋある。Lasworks patent (U, S, Pat 2215)
059.2221709), borosilicate glass made from boric acid, alkali metal oxide, silica sand, etc. as main raw materials is heat treated at a temperature of several hundred degrees to form a silica sand glass phase and a boric acid and alkali metal oxide. The phase is separated into a glass phase rich in substances. Next, by treating this glass with an acid solution or hot water, the glass phase rich in boric acid and alkali gold mK was eluted, resulting in a glass that retained its original shape and was rich in silicic acid components. [Problem to be solved by the invention] However, in the above-mentioned prior art, boric acid and alkali gold
Because the pores are formed by eluting the K-rich glass phase, it is impossible to form uniform pores for glass with a thickness of several centimeters, and it is difficult to obtain bulk materials. The problem is that it is difficult to Therefore, the present invention aims to solve these problems, and its purpose is to create a porous material with a thickness of several centimeters, uniform pores, and a very sharp distribution. There are several companies that provide methods for manufacturing glass.
本発明の多孔質ガラス製造方法は金属アルフキシトを原
料とするゾル−ゲル法により、粒径のそろった球状のシ
リカ粒子を合成し、その粒子を沈殿させ固めた後、焼結
することを特徴とする。The porous glass manufacturing method of the present invention is characterized by synthesizing spherical silica particles with uniform particle sizes by a sol-gel method using metal alphoxide as a raw material, and sintering the particles after precipitating and solidifying them. do.
以下に実施例を詳細に説明する。 Examples will be described in detail below.
実施例１゜
テトラエトキシシラン１００ ｍｆｌにエタノールを１
１００ｍｆｉとアンモニア水を３０ｍ℃加え、１時間攪
拌しその後５時間放置し直径５００オングストロ一ム程
度の単分散の球状シリカを得る０この粒子の混入した溶
液をロータリーエバポレーターで濃縮し溶液の体積で５
分の１程度にする。次にテトラエトキシシラン５０ｍ２
に０．０１．ｌ定の塩酸を１００？ＦＩＩ／、加え激し
く攪拌し加水分解し、このゾルと前述の濃縮液を加えｐ
Ｈを２〜３に調整した後、φ２０Ｘｈ５０ｍのポリプロ
ピレン製の容器に入れ密閉し１０〜１５度で保温しなか
ら防臭台の上で２〜３ケ月放置する。粒子が沈殿したと
ころで容器に１０〜３０％の穴を開け３０〜４０麿で乾
燥する。乾燥が終了したところで１０００〜１２００℃
で焼成し多孔質ガラスを得る。得られた多孔質ガラスの
細孔径分布を第１図忙示す。Example 1: Add 1 ethanol to 100 mfl of tetraethoxysilane.
Add 100mfi and ammonia water at 30m℃, stir for 1 hour, and then leave for 5 hours to obtain monodisperse spherical silica with a diameter of about 500 angstroms.The solution containing the particles is concentrated using a rotary evaporator to reduce the volume of the solution to 5
Reduce it to about 1/2. Next, 50m2 of tetraethoxysilane
to 0.01. l constant hydrochloric acid 100? Add FII/, stir vigorously to hydrolyze, add this sol and the above-mentioned concentrated solution, and
After adjusting H to 2 to 3, the container is placed in a polypropylene container measuring 20 m in diameter and 50 m in height, sealed, kept warm at 10 to 15 degrees, and left on a deodorizing table for 2 to 3 months. Once the particles have precipitated, make a 10-30% hole in the container and dry for 30-40 minutes. 1000-1200℃ after drying
to obtain porous glass. The pore size distribution of the obtained porous glass is shown in Figure 1.
実施例２゜
テトラエトキシシラン１００ ｍｆ）、にエタノールを
１１００ ｎｅｆｔとアンモニア水を７０ｍ２加え、１
時間攪拌しその後５時間放置し直径１０００オングスト
ローム程度の単分散の球状シリカを得る。以下実施例１
と同様に行ない多孔質ガラスを得る。Example 2 1100 m2 of ethanol and 70 m2 of aqueous ammonia were added to 100 mf of tetraethoxysilane.
The mixture was stirred for an hour and then left to stand for 5 hours to obtain monodisperse spherical silica with a diameter of about 1000 angstroms. Example 1 below
Proceed in the same manner as above to obtain porous glass.
得られた多孔質ガラスの細孔径分布を第２図に示すＯ
実施例３゜
テトラエトキシシラン１００ ｍＮにエタノールを１１
００ ｖａｎとアンモニア水を７０ ｙｎｊ！加え、１
時間攪拌しその後５時間放置し直径３０００オングスト
ロ一ム程度の単分散の球状シリカを得る。以下実施例１
と同様に行ない多孔質ガラスを得る。The pore size distribution of the obtained porous glass is shown in Figure 2.
00 van and ammonia water for 70 ynj! In addition, 1
The mixture was stirred for an hour and then allowed to stand for 5 hours to obtain monodisperse spherical silica with a diameter of about 3000 angstroms. Example 1 below
Proceed in the same manner as above to obtain porous glass.
得られた多孔質ガラスの細孔径分布を第３図に示すＯ
実施例４゜
テトラエトキシシラン１００ ？？Ｉｆｌ Ｉｃエタノ
ールを１１００ ｍ（１，とアンモニア水を７０ ｍＮ
加え、１時間攪拌しその後５時間放置し直径５０００オ
ングストロ一ム程度の粒子を得る０以下実施例１と同様
に行ない多孔質ガラスを得る。得られた多孔質ガラスの
細孔径分布を第４図に示す。The pore size distribution of the obtained porous glass is shown in FIG. 3. Example 4 Tetraethoxysilane 100? ? Ifl Ic ethanol at 1100 m (1, and aqueous ammonia at 70 mN)
The mixture was stirred for 1 hour and then left for 5 hours to obtain particles with a diameter of about 5,000 angstroms.The procedure in Example 1 was repeated to obtain porous glass. The pore size distribution of the obtained porous glass is shown in FIG.
以上述べたように発明によれば、金属アルフキシトを原
料とするゾル−ゲル法により、粒径のそろった球状のシ
リカ粒子を合成し、その粒子を沈殿させ固めた後、焼結
することにより、バルク状であり細孔径分布が非常にシ
ャープである多孔質ガラスを得ることができるという効
果を有する０As described above, according to the invention, spherical silica particles with uniform particle sizes are synthesized by the sol-gel method using metal alphoxide as a raw material, and after the particles are precipitated and solidified, they are sintered. 0, which has the effect of being able to obtain porous glass that is bulk-like and has a very sharp pore size distribution.
第１図は本発明における実施例１の細孔径分布を示す図
。
＠２図は本発明における実施例２の細孔径分布を示す図
。
第３図は本発明における実施例３の細孔径分布第４図は
本発明における実施例４の細孔径分布を示す因。
以 上
出願人 セイコーエプソン株式会社
１０ 、ω １００Ｑ
軸：！ＩＬ径（，０
第１−図
Ｉｏ １ｃｏ ｒｏｏ。
細孔径ｒＡ）
第２図
１０ １００ ｔαり
細孔径（１）
＋０ １０１） Ｉｏｏ。
細孔径（／４′）
第４図FIG. 1 is a diagram showing the pore size distribution of Example 1 of the present invention. @2 Figure is a diagram showing the pore size distribution of Example 2 of the present invention. FIG. 3 shows the pore size distribution of Example 3 according to the present invention. FIG. 4 shows the pore size distribution of Example 4 according to the present invention. Applicant: Seiko Epson Corporation 10, ω 100Q axis:! IL diameter (,0 Fig. 1 Io 1co roo. Pore diameter rA) Fig. 2 10 100 tα pore diameter (1) +0 101) Ioo. Pore diameter (/4') Figure 4
Claims (1)
径のそろった球状のシリカ粒子を合成し、その粒子を沈
殿させ固めた後、焼結することを特徴とする多孔質ガラ
ス体の製造方法。A method for producing a porous glass body, which comprises synthesizing spherical silica particles of uniform particle size by a sol-gel method using a metal alkoxide as a raw material, precipitating and solidifying the particles, and then sintering the particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7326186A JPS62230636A (en) | 1986-03-31 | 1986-03-31 | Production of porous glass article |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7326186A JPS62230636A (en) | 1986-03-31 | 1986-03-31 | Production of porous glass article |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62230636A true JPS62230636A (en) | 1987-10-09 |
Family
ID=13513057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7326186A Pending JPS62230636A (en) | 1986-03-31 | 1986-03-31 | Production of porous glass article |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62230636A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01183445A (en) * | 1988-01-13 | 1989-07-21 | Shimadzu Corp | Structural component and production thereof |
-
1986
- 1986-03-31 JP JP7326186A patent/JPS62230636A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01183445A (en) * | 1988-01-13 | 1989-07-21 | Shimadzu Corp | Structural component and production thereof |
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